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A method for rapidly preparing high-purity hydroxy-α-sanshool

A technology of sanshool and hydroxyl, applied in the field of rapid preparation of high-purity hydroxy-α-sanshool, can solve the problems of long time, unstable results, poor repeatability, etc., and achieve the effects of improving purity, simple operation and low cost

Active Publication Date: 2019-01-15
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

03132341.3 discloses a process for separating the numbing components of prickly ash using supercritical fluid technology. This process requires high equipment operation technology, and the prepared numbing components are preliminary extracts. This type of method requires strong operating experience. The reproducibility is extremely poor, the result is unstable, and it takes a long time, and the prepared numbing component is a preliminary extract, which can only be used in industrial production. As a raw material for food and medicine, it is not suitable as a standard for quantitative numbing
And 201210175527.9 uses thin-layer chromatography to extract high-purity hydroxyl sanshool from Zanthoxylum bungeanum oil. Although this gap has been filled, the chromatographic column of liquid chromatography is still used in the preparation process, and the preparation cost increases.

Method used

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  • A method for rapidly preparing high-purity hydroxy-α-sanshool
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  • A method for rapidly preparing high-purity hydroxy-α-sanshool

Examples

Experimental program
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Effect test

Embodiment 1

[0024] (1) Take 30 mL of red prickly ash oil, add methanol at a volume ratio of 1:20, use a constant temperature oscillator at 40°C for 1 hour, rotate at 160 rpm, and then sonicate for 5 minutes, transfer the extract into a centrifuge tube and centrifuge at 4000 r / min Take the supernatant after 15 min;

[0025] (2) Extract the supernatant with n-hexane, the ratio of solid to liquid is 1:2, extract 3 times, pass the extracted subnatant through an alkaline aluminum oxide column, and pass the obtained chromatographic solution through a 0.22 μm organic filter membrane , and finally the filtrate was evaporated to dryness under reduced pressure at 45°C (vacuum degree 0.09Mpa) with a rotary evaporator for 2 hours to obtain a crude extract;

[0026] (3) Dissolve 10mg of the crude extract in 20mL of chromatographic grade methanol, put it into a serum bottle, and irradiate it with ultraviolet light. The time is 2 hours. After the irradiation is over, use a rotary evaporator at 45°C (va...

Embodiment 2

[0028] (1) Take 30 mL of red prickly ash oil, add methanol at a volume ratio of 1:20, use a constant temperature oscillator at 40°C for 1 hour, rotate at 160 rpm, and then sonicate for 5 minutes, transfer the extract into a centrifuge tube and centrifuge at 4000 r / min Take the supernatant after 15 min;

[0029] (2) Extract the supernatant with n-hexane, the ratio of solid to liquid is 1:2, extract 3 times, pass the extracted subnatant through an alkaline aluminum oxide column, and pass the obtained chromatographic solution through a 0.22 μm organic filter membrane , and finally the filtrate was evaporated to dryness under reduced pressure at 45°C (vacuum degree 0.09Mpa) with a rotary evaporator for 2 hours to obtain a crude extract;

[0030] (3) Dissolve 10mg of the crude extract in 20mL of chromatographic grade methanol, put it into a serum bottle, and irradiate it with ultraviolet light. The time is 4 hours. After the irradiation is over, use a rotary evaporator at 45°C (va...

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Abstract

The invention discloses a method for rapidly preparing high-purity hydroxyl-alpha-sanshool. The method adopts three key steps of oscillation extracting at a constant temperature, extracting by n-hexane and ultraviolet radiation treatment. In addition, the preparation method does not need a special instrument such as a preparation-type or semi-preparation-type high-performance liquid-performance chromatograph, so that compared with the traditional column chromatography, the preparation method is simpler, shorter in time and low in cost, so that the method can be used by an ordinary laboratory and people with general operation skill to prepare the high-purity hydroxyl-alpha-sanshool toperform neededexperiments, and the working efficiency is greatly improved.

Description

technical field [0001] The invention relates to the field of separation and purification of natural products, in particular to a method for rapidly preparing high-purity hydroxy-α-sanshool. Background technique [0002] Zanthoxylum bungeanum oil is directly soaked Zanthoxylum bungeanum in edible oil or extracted with organic solvent, supercritical CO 2 The seasoning oil with hemp flavor is made by mixing the pepper oleoresin prepared by extraction and other methods with edible oil in an appropriate amount. The processing of Zanthoxylum bungeanum oil greatly reduces the loss of active ingredients and microbial contamination caused by Zanthoxylum bungeanum during storage and sales, and solves the inconvenience caused by Zanthoxylum bungeanum and Zanthoxylum powder to cooking and eating, so it is more and more popular among consumers. However, the current market for pepper oil is not regulated, and most product labels only indicate raw materials, while the content of numbing s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/24C07C233/20
CPCC07C231/24C07C233/20
Inventor 刘福权赵志峰靳岳
Owner SICHUAN UNIV